Process of treating spent adsorbents



Dec. 6, 1932. l. K. FULLER l PROCESS OF TREATING SPENT ADSORBENTS FiledSept. 27. 1929 2 Smets-Sheet. 1

Dec. 6, 1932. K. FULLER 1,890,255

PROCESS 0F TREATING SPENT ADSORBENTS Filed Sept. 27, 1929 2 Sheets-Sheet2 l Patented Dee. 6, T932 i `1,890,255

-UNITED sTATEs PATENT OFFICE IRA .K. FULLER, F vCLEAN', NEW vYORK;ASSIGNOR, BY MSNE ASSIGNMENTS, T0 ACONTACT FILTRATION COMPANY,'ACORPORATION 0F CALIFORNIA rnocEss or TREATTNG srENT Anson-ennuis i IApplication mea september a7, 1929. serial No. 395,595.

This invention relates particularly to the hopper, the spent adsorbentto-be reactivated treatment' of adsorbents, such as vactivated is mixedwith a solvent for the oil,'this solvent clay, which have been used indecolorizing being conveniently and preferably gasoline oil. Suchmaterial, after separation from of low aromatic content such as thatobtained the bulk of the treatedA oil,` still contains a in thedistillation of Pennsylvania crude. .0' certain amount of oil whichcannot be re- The mixture of gasoline and spent adsorbent v 1 moved fromit in the filtering operation, and (clay) is paossed to a heater by wayof a its activity has been lost through adsorption heat exchanger, thisheat exchanger reof the gummy or resinous coloring matter heating theincoming mixture throught erwhich it is its function to remove from themal contact with the heated mixture issuing oil. To save the residualoil and restore the from the heater. The heater may be ay tube utilityof the clay, it is desirable to first' restill or any otherconvenient'type of conmove the oil, by the use of a suitable solvent,tinuous heater, in which the mixture of clay and thereafter to removetheadsorbed matand solvent is constantly agitated during the .ter by asolvent adapted for this purpose. heating. The clay-solventmixtureis'heated 60 The object of this invention is to provide untilsolution of the oil, as shown by trial,

a pIOCeSS, for the purpose deSCribed,iI1 Which is complete.A The mixturethen passes to an the removal of adsorbed matter from the agitating orsolution mixing tank, where it is adsorbent or clay may beaccomplished'with further agitated,l f e eCOIlQmy, but with suchcompleteness that a The mixture next passes to a filter-press of 65bulflllng 0PeI310I1, f0I the PUIPOSB 0f 1'6- standard construct-ion, thetypepdesignated activation, may be dispensed with, or if used, 0n thedrawings being known as the Oliver will not lnvolve contamination ofthe` clay press, although any type maybe employed.

with residues 0f combustion- The Oliver press comprises a. tank or liq-A I have found that the desired result may `uid-tight receptacle, inwhich there is placed 7o be Seeuied by Washing the edeorbed material arevolving drum .carrying the .filter cloth,

' fromme Clay by a: process Whlch tngolves the the drum being sopositioned that it is parstep of rst .mum-1g the .Clay Wlt' enoughtially immersed in the liquid being filtered. solvent to bruigsubstalftlauy 31.1 of the ad" The drum is divided into a number of com-Sorbed matter Into Solutlon heatmg and agl' partments, and. is connectedwith a vacuum 75 tating the mixture until solution is pracv n 1n suchmanner that the compartments willtically complete, filtering the clay from tnu be successively .exhausted and the liquid mixture and thenwashlno" from the filter4 cake, the small amountofbeolution remain-Adrawn through the filter dothby the Suchen ing therein, by percolatingthrough the cake ehe eehdmetr olflgmauy Suspended,v 1u the' 0 anadditional amount of fresh solvent. hqlud bemg deposlted upon theexerlor sur' The complete process may be carried out face of the drum asa cake, which 1s removed y in a plantl comprising two substantiallysimby a Statlouary Scraper mounted adlaeeut t0 ilar sets. of apparatusfor performing the two the dI'lUIL 40 respective operations of oilremoval and re- The PITeSS (Hilke, freed fIOIIl entrallled 011 85activation, and in the 'accompanying drawbut still containing gasolineis conveyed to ings Fig. l is a flow sheet representing the hoppers.From these hoppersvit is'taken to oil-removal apparatus, `and Fig. 2repre axdryer, which preferably is of a stationary sents thereactivating apparatus. v drum type, and heated by a convenientsourceBeginning in'Figure 1 'with the mixing of heat. The vapors from thedryer are con- 90 hot material .issuing densed and the residual gasolinein the cake thus recovered.

The dried clay, discharged from the dryer through a suitable hopper "orvalve to trap any vapor, is ready for reactivation,

For this purpose apparatus as outlined on Figure 2 is employed, thisapparatus being analogous to that of Fig. 1. The oil-freed clay iscarried vfrom the dryer of Fig. 1 to an elevator and then dischargedinto a mixing hopper where it is mixed with a reactivating solvent.

A number of solvents may be employed, as, for example, benzol, or 'famixture of benzol with methyl-ethyl ketone. The mixture oi gum solventand clay passes through the heat y exchanger (Figure 2),

then through the heater, Where the mixture is heated to facilitate thesolutionof the gums 'and resins, the incoming mixture of clay and gumvsolvent being preheated by thermal contact with the lfrom the heater.The material from the'heater, which now is composed of the claysubstantially freed from its gum and resin content, together with thesol-x vent and the gums and resinsin solution, passes to a` solution.mixing that described before, and resin solvent may be added if desired.From this tank, themixture is transferred to a lter-press, vwhich may bealso, conveniently,` of the Oliver type.

In order to carry out the present process this press is equipped withmeans for spraying solvent upon the cake formed in the press, and thesuction boxes then act to draw the l. 4solvent through the cake, thuswashing out the solution of adsorbed matter which would By the use of bemade leave the clay practically otherwise remain in the cake. a seriesof spray jets this action may so complete as to free from solublematter. f

The washed clay cake is scraped from the drum and again conveyed toreceiving hoppers,as previouslyl described in connection with the oilextraction operation, then conveyed to a dryer, conveniently of the typedescribed in connection with the extraction stage, the clay being dried,as before, by any convenient source of heat. As shown in Figure 2, fromthe dryer the activated clay is conveyed to an elevator, from which itis deposited and sent to storage.

tank, similar to where additional gum tion of adsorbed matter therefrom.

p 2. A process for reactivating spent adsorbent from an o il contactingoperation, which process comprises treating the adsorbent `freshxsolvent to wash the remaining solufor removal of oil, mixing theadsorbent with l a solvent for adsorbed matter and agitating and heatingthe mixture until solution is substantially complete, ltering theadsorbentrom the mixture, and passing, thro-ugh the y filter cake, afurther quantity of'fres'h solvent to Wash the remalning solution ofvad#rsorbed. matter therefrom.

IRA K. FULLER.

What I claim as my inventionv and desire to secure by Letters Patent is:

1. A process for reactivating spent adsorbd ent from an oil .contactingoperation, which process comprises treating the adsorbent with an oilsolvent for removal of oil, drying the adsorbent, mixing the driedadsorbent with a solvent for adsorbed matter, filtering the

